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Method utilizing micro-channel to prepare tris(2-chloroethyl)phosphite

A technology of phosphite and chloroethyl, which is applied in the field of preparation of tri-phosphite, can solve problems such as low production efficiency, instability, and limited heat exchange area, and achieve air isolation, avoid oxidation and hydrolysis, and low cost effect

Active Publication Date: 2014-10-29
SHAOXING EASTLAKE HIGH TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the esterification reaction of phosphorus trichloride and ethylene oxide has the following problems in common enamel reactors: (1) Since the above-mentioned esterification reaction is a strong exothermic reaction, the heat transfer area of ​​common enamel reactors Very limited, which restricts the ventilation rate of ethylene oxide. In a 2000-liter reactor, the ventilation rate of ethylene oxide can only reach 5kg / h~15kg / h, and a batch of tri-(2-chloroethane Base) phosphite needs 110 hours, the production efficiency is very low
(2) The tri-(2-chloroethyl) phosphite product itself is not very stable, and it will polymerize and produce side reactions if it stays at a temperature of 45 ° C to 50 ° C for a long time. At the same time, the raw material phosphorus trichloride is in contact with humid air for a long time Also can produce a series of side reactions such as oxidative hydrolysis, therefore, adopt the above-mentioned method to produce the content that obtains tri-(2-chloroethyl) phosphite and can only reach about 90%, seriously restricted the content of the former medicine of ethephon

Method used

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Embodiment 1

[0026] The microchannel reaction device is a two-level series (that is, two groups of microchannel reactors are connected in series), and each stage of microchannel reactors consists of 200 Composed of pipes, the outer diameter of the reactor is 600mm, and the length is 2000mm;

[0027] Phosphorus trichloride and ethylene oxide are pumped continuously into the pipeline premixer (by In static mixing pipeline composition), the mass flow rate of phosphorus trichloride is controlled to be 100kg / h, and the mass flow rate of ethylene oxide is 100kg / h; Enter the microchannel reaction device in two series series, carry out exothermic reaction in the microchannel reaction device, and open the refrigerant cooling equipment (refrigerant is 7# industrial grade white oil) coupled to the microchannel reactor at the same time for cooling, and the temperature of the refrigerant is - 16 ~ 10 ℃, control (adjusted by the outlet of the back pressure valve in the last section of the microchanne...

Embodiment 2

[0029] The microchannel reactor is a four-level series (that is, four groups of microchannel reactors are connected in series), and each level of microchannel reactor consists of 250 The pipe is composed of a reactor with an outer diameter of 600mm and a length of 2000mm.

[0030] Phosphorus trichloride and ethylene oxide are pumped continuously into the pipeline premixer (by Static mixing pipeline composition), control the mass flow of phosphorus trichloride to be 300kg / h, and the mass flow of ethylene oxide to be 300kg / h. The mixture of phosphorus trichloride and ethylene oxide pre-mixed by the pipeline mixer enters the four-stage series microchannel reactor, and the exothermic reaction is carried out in the microchannel reactor, and the coupling with the microchannel reaction system is opened at the same time. Refrigerant cooling equipment (refrigerant is 7# industrial grade white oil) for cooling, the temperature of the refrigerant is -16 ~ 10 ℃, and the temperature of th...

Embodiment 3

[0032] The microchannel reactors are six stages in series (that is, six groups of microchannel reactors are connected in series), and each stage of microchannel reactors consists of 300 The pipe is composed of a reactor with an outer diameter of 600mm and a length of 2000mm.

[0033] Phosphorus trichloride and ethylene oxide are pumped continuously into the pipeline premixer (by Static mixing pipeline composition), control the mass flow of phosphorus trichloride to be 500kg / h, and the mass flow of ethylene oxide to be 500kg / h. The mixed solution of phosphorus trichloride and ethylene oxide pre-mixed by the pipeline mixer enters the six-stage series microchannel reaction device, and the exothermic reaction is carried out in the microchannel reaction device, and the coupling with the microchannel reactor is opened at the same time. Refrigerant cooling equipment (refrigerant is 7# industrial grade white oil) for cooling, the temperature of the refrigerant is -16 ~ 10 ℃, and ...

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Abstract

The invention discloses a method utilizing micro-channel to prepare tris(2-chloroethyl)phosphite. The method comprises the following steps: taking phosphorus trichloride and ethylene oxide as the raw materials, and then carrying out reactions in a micro-channel reaction system composed of a micro-channel reaction device which is formed by coupling a pipeline-type pre-mixer and cooling-medium cooling equipment; and specifically comprises the following steps in sequence: first continuously pumping phosphorus trichloride and ethylene oxide into a pipeline-type pre-mixer to carry out premixing, then introducing the mixture into a micro-channel reaction device, starting the cooling-medium cooling equipment of a micro-channel reaction system, and collecting the effluent liquid from the micro-channel reaction device after the reactions finish, wherein the effluent liquid is tris(2-chloroethyl)phosphite. The method can largely increase the esterification product content, the production efficiency is increased by 500 to 1000 times compared to that of common tank reactor, and the standing time of the esterification products in the reactor is reduced from 110 hours to dozen minutes.

Description

(1) Technical field [0001] The invention relates to a method for preparing tris-(2-chloroethyl)phosphite, in particular to a method for preparing tris-(2-chloroethyl)phosphite using microchannel reaction technology. (2) Background technology [0002] Tris-(2-chloroethyl)phosphite is an important intermediate for the production of plant growth regulator ethephon. At present, the commonly used production method in China is: put phosphorus trichloride into the reactor, and vaporize ethylene oxide Then pass it into liquid phosphorus trichloride for reaction, control the temperature in the kettle at 45°C to 50°C, the reaction equation is: [0003] [0004] The above-mentioned esterification reaction is a strongly exothermic reaction. At present, the esterification reaction of phosphorus trichloride and ethylene oxide has the following problems in common enamel reactors: (1) Since the above-mentioned esterification reaction is a strong exothermic reaction, the heat transfer ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/141
CPCC07F9/1411
Inventor 季国炎丁成荣张国富季盛季国尧季小英杨华东
Owner SHAOXING EASTLAKE HIGH TECH CO LTD
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